ASTM D1135-86(2009)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D1135 − 86 (Reapproved2009)
Standard Test Methods for
Chemical Analysis of Blue Pigments
This standard is issued under the fixed designation D1135; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 2. Referenced Documents
1.1 These test methods cover procedures for the chemical
2.1 ASTM Standards:
analysis of blue pigments known commercially as iron blue,
D280 Test Methods for Hygroscopic Moisture (and Other
copper phthalocyanine blue, and ultramarine blue.
Matter Volatile Under the Test Conditions) in Pigments
D1193 Specification for Reagent Water
1.2 The analytical procedures appear in the following order:
D1208 Test Methods for Common Properties of Certain
Sections
Pigments
I RON BLUE P IGMENTS
D2448 Test Method for Water-Soluble Salts in Pigments by
Measuring the Specific Resistance of the Leachate of the
Identification 6
Moisture by the Brabender Moisture Tester 7 and 8
Pigment
Moisture by Toluene Distillation 9
E11 Specification for Woven Wire Test Sieve Cloth and Test
Water-Soluble Matter by Extraction 10
Sieves
Water-Soluble Salts by Electrical Conductivity 11
Detection of Acid-Insoluble Extenders 12 and 13
Detection of Acid-Soluble Extenders 14 to 17
3. Significance and Use
Detection of Organic Colors and Lakes 18
3.1 These test methods are suitable for determining if
C OPPER PHTHALOCYANINE BLUE PIGMENTS
impurities are present and establishing that the required pig-
Identification 19
ments are present. These test methods may be used for
Moisture and Other Volatile Matter 20
manufacturing quality control.
Detection of Basic Dye Derivatives 21
Detection of Other Organic Coloring Matter 22
Detection of Ultramarine Blue 23
4. Purity of Reagents and Water
Detection of Iron Blue 24
4.1 Purity of Reagents—Unless otherwise indicated, it is
U LTRAMARINE BLUE
intended that all reagents shall conform to the specifications of
Identification 25
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
Moisture and Other Volatile Matter 26
cal Society, where such specifications are available. Other
Water-Soluble Matter 27
Detection of Basic Dye Derivatives 28 grades may be used, provided it is first ascertained that the
Detection of Other Organic Coloring Matter 29
reagent is of sufficiently high purity to permit its use without
1.3 The values stated in SI units are to be regarded as
lessening the accuracy of the determination.
standard. No other units of measurement are included in this
4.2 Purity of Water—Unless otherwise indicated, references
standard.
towatershallbeunderstoodtomeanreagentwaterconforming
1.4 This standard does not purport to address the safety
to Type II of Specification D1193.
concerns associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety and health
practices and determine the applicability of regulatory limita-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tions prior to use.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 3
These test methods are under the jurisdiction of ASTM Committee D01 on Reagent Chemicals, American Chemical Society Specifications, American
Paint and Related Coatings, Materials, and Applications and are the direct Chemical Society, Washington, DC. For suggestions on the testing of reagents not
responsibility of Subcommittee D01.31 on Pigment Specifications. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved June 1, 2009. Published June 2009. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1950. Last previous edition approved in 2004 as D1135 – 86 (2004). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D1135-86R09. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1135 − 86 (2009)
5. Preparation of Sample
5.1 Mix the sample thoroughly and take a representative
portion for analysis. Reduce any lumps or coarse particles to a
fine powder by grinding.
5.2 Grind extracted pigments to pass a No. 80 (180-µm)
sieve. Discard any skins that do not pass through the sieve.
Mix the finely ground pigment thoroughly.
Detailed requirements for this sieve are given in Specification E11.
IRON BLUE
(Prussian Blue, Chinese Blue, Milori Blue)
NOTE 2—The dried pigment is very hygroscopic. In order to obtain
IDENTIFICATION
consistentresults,thespecimenpositionmustnotbechangedandtheoven
door must not be opened.
6. Procedure
8.3 Calculation and Report—Plot time against percent loss
6.1 To approximately 0.1 g of pigment in a 50-mL beaker,
in weight on rectilinear cross-section paper. Extrapolate the
add15mLofNaOHsolution(50g/L).Heattoboiling.Inafew
linear portion of the curve to zero time. That portion beyond
minutes the blue color should be completely destroyed, giving
about 2 h will be essentially linear. Report the percent loss in
initsplacethecharacteristicreddishbrownprecipitateofferric
weight at the extrapolated zero time as the percent moisture in
hydroxide.Add HCl (1+1) until faintly acid to litmus.The iron
the pigment.
blue should be reformed, yielding again the characteristic blue
NOTE 3—The pigment undergoes a slight loss in weight due to
color.
decomposition during the heating. The method of plotting and extrapola-
tion corrects for this loss.An approximate value for moisture content may
NOTE 1—If the NaOH treatment does not completely destroy the blue
be obtained by taking the reading at the end of the first hour’s heating.An
color, the evidence is strong that a foreign pigment is present. If this
occasional pigment may decompose rapidly at the oven temperature. In
occurs, it is best to filter the alkaline solution, weakly acidify the filtrate
such cases, determine moisture by the toluene distillation method (Section
with HCl (1+1), and add approximately 2 mL of a ferric salt solution
9).
(ferric sulfate or ferric alum (20 g/L)). The formation of a blue precipitate
established the pigment as consisting, at least in part, of iron blue.
MOISTURE BY TOLUENE DISTILLATION
MOISTURE BY THE BRABENDER MOISTURE
9. Procedure
TESTER
9.1 Determine the moisture content in accordance with
7. Apparatus
Sections 7 and 8 of Test Method D1208, but using 25 g of
pigment and 200 mL of toluene and adjusting the calculation
7.1 Brabender Moisture Tester—The Brabender moisture
accordingly.
tester (Fig. 1) consists of a constant-temperature oven with
weighing apparatus attached. Specimens placed in the oven
WATER-SOLUBLE MATTER BY EXTRACTION
may be weighed without opening the oven door or removing
the specimen from the oven, as the balance scale is calibrated
10. Procedure
to read directly in percent of moisture.
10.1 Determine whether or not the pigment is easily wet by
water at room temperature by adding a little to some water in
8. Procedure
a beaker. If it tends to float on top of the water with very little,
if any, tendency to sink to the bottom or disperse throughout
8.1 Set the temperature control at 160°C and allow the oven
the solution, even after agitation, it contains a hydrophobic
to reach this temperature before checking or making any
treating agent.
weighing. Check the scale by placing a sample dish containing
9.200 g standard analytical balance weights in the oven. The
10.2 Weigh to 1 mg about 2.5 g of the pigment into a
apparatus should read 8.0 % moisture. If it does not, adjust to
250-mL volumetric flask. If the pigment is hydrophobic as
a reading of 8.0 % by turning either the right hand or left hand
tested above, moisten thoroughly with a few mL of ethyl
foot screw.
alcohol (Note 4). If the pigment is easily wet with water, no
alcohol is necessary. Fill the flask about half full with water
8.2 Weigh 10.000 g of the sample into the aluminum dish
and shake to disperse the pigment thoroughly. Fill to the mark
and place in the oven. For a series of specimens, all should be
and again shake. Allow to remain at room temperature for not
placed in the oven at as nearly the same time as possible. No
less than 15 h, shaking from time to time, preferably with an
specimen should occupy the position directly in front of the
automatic shaking device.
door.Weigh the specimen at the end of each hour for 5 h.After
each weighing, return the specimen to its original place in the
NOTE 4—Ethyl alcohol denatured with acetone (Formula No. 23A) or
oven. denatured with methyl alcohol (Formula No. 3A) has been found suitable.
D1135 − 86 (2009)
FIG. 1 Brabender Moisture Tester
10.3 Let settle, filter through a dry filter paper, and discard 13. Procedure
the first 20 mL of the filtrate. Transfer 100 mL of the clear
13.1 Ignite about 1 g (weighed to 0.1 mg) of the sample at
filtrate to a weighed dish, and evaporate to dryness on a steam
a low temperature, just enough to decompose the last trace of
bath. Dry for1hinan oven at 105 6 2°C, cool, and weigh.
pigment but not high enough to render the iron difficultly
10.4 Calculation—Calculate the percent of water-soluble
soluble in HCl (Note 5). Cool, and add 15 mL of HCl (sp gr
matter as follows:
1.19) and a few drops of bromine. Cover with a watch glass
and evaporate to a sirup. Add about 15 mL of water, and boil.
Water 2 soluble matter,% 5 grams of residue 3100
It may be necessary to add a drop or two of HCl to effect
WATER-SOLUBLE SALTS BY ELECTRICAL
complete solution of the ferric iron residue. Filter and wash
CONDUCTIVITY
with hot water. Save the filtrate for the determination of
alumina hydrate (Section 16).
11. Procedure
NOTE 5—The ignition can conveniently be carried out in a 250-mL
11.1 Determine water-soluble salt content in accordance
beaker or a porcelain dish over a free flame. Oxidation of the specimen is
with Test Method D2448.
evidenced by a dull glowing.While being heated, it is advisable to roll the
specimen around in the beaker or dish exposing all of the surface to the
DETECTION OF ACID-INSOLUBLE EXTENDERS
oxygen of the air.Amoderately low flame should be used and the ignition
is complete when the specimen ceases to glow and acquires a uniform
12. Scope brown color.
12.1 Acid-insolubleextendersincludebariumsulfate,silica, 13.2 Aresidue of less than 3 mg that appears as small black
and silicates. Alumina may also be found, in part, with this specks can be neglected, since quite frequently a small amount
group. of
...